HRID1282185

反应详情

EQUATION

反应方程式

HRID 1282185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-(4-chloromethylphenylmethyl)acetamide (0.9 g), 1-(4-dimethylamino-6-methoxypyrimidin-2-yl)piperazine (1.1 g) and potassium carbonate (1.0 g) in dimethylformamide (10 ml) was stirred at 80° C. for 8.5 hr. The reaction mixture was poured into water (100 ml) and extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated to give a brown oil (1.9 g). The obtained brown oil was purified by silica gel column chromatography (developing solvent; chloroform:methanol=9:1) to give a yellow oil (1.6 g). The obtained yellow oil was crystallized from ethyl acetate/hexane (1:1, 20 ml) to give the title compound (1.0 g) as pale-yellow crystals.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated